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Luminescent semiconductors are the key material in a host of optoelectronic devices, including solar cells, light-emitting diodes, and x-ray scintillators, and have been discovered at an increasing rate over the last decades. To optimize any device, a luminescent semiconductor’s photophysics must be understood and its loss processes minimized. Several accessible spectroscopic techniques exist, which can together give all relevant photophysical information, namely, UV-Vis spectroscopy, photoluminescence quantum efficiency, and time-resolved photoluminescence. However, these measurements are often poorly used, incorrectly fitted, or important information is missed. Here, we present best practices in applying these techniques to characterize luminescent semiconductors with unknown photophysical properties. We highlight which information can be obtained from each measurement, when it is appropriate to apply different mathematical models, and give examples from a range of semiconductors. This work will help to standardize and streamline the characterization of luminescent semiconductors, enabling more efficient devices.